CN104597013B - A kind of fluorescent spectrometry surveys the method that cholesterol level differentiates gutter oil - Google Patents
A kind of fluorescent spectrometry surveys the method that cholesterol level differentiates gutter oil Download PDFInfo
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- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 title claims abstract description 172
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004611 spectroscopical analysis Methods 0.000 title claims abstract description 7
- 235000012000 cholesterol Nutrition 0.000 claims abstract description 77
- 239000003921 oil Substances 0.000 claims abstract description 56
- 235000019198 oils Nutrition 0.000 claims abstract description 56
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 21
- 239000008158 vegetable oil Substances 0.000 claims abstract description 21
- 238000007127 saponification reaction Methods 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 230000008859 change Effects 0.000 claims abstract description 4
- 230000005284 excitation Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 76
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 32
- 238000012360 testing method Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 11
- 238000002189 fluorescence spectrum Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000013517 stratification Methods 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 5
- 239000008157 edible vegetable oil Substances 0.000 claims description 3
- 239000000344 soap Substances 0.000 claims description 3
- 239000011550 stock solution Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 19
- 239000010775 animal oil Substances 0.000 abstract description 5
- 239000004519 grease Substances 0.000 abstract description 2
- 238000004451 qualitative analysis Methods 0.000 abstract description 2
- 238000007664 blowing Methods 0.000 abstract 1
- 238000004445 quantitative analysis Methods 0.000 abstract 1
- 241000183294 Scleropages formosus Species 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000007705 chemical test Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
- 238000004851 dishwashing Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The invention discloses a kind of method that fluorescent spectrometry surveys cholesterol level discriminating gutter oil, animal oil can be typically mixed into ditch oil, contains grease in animal oil, there can be the cholesterol more than common vegetable oil, so start with terms of cholesterol, and the effective means of detection gutter oil.Cholesterol has fluorescence in itself, wherein maximum fluorescence excitation wavelength lambda ex=266nm, maximum emission wavelength λ em=280nm, configure a series of standard cholesterol solution of concentration, standard curve of the fluorescence intensity with change in concentration can be made, carries out cholesterol quantitative determination.Gutter oil is added into KOH and ethanol carries out saponification, n-hexane extraction is then added, is passed through N2After air-blowing is dry, qualitative and quantitative analysis is carried out to sample using fluorescent spectrometry.
Description
Technical field
The present invention relates to gutter oil detection technique, more particularly to it is a kind of with XRF cholesterol detection content come
Differentiate the method for gutter oil.
Background technology
The discrimination method of gutter oil is also a lot, and gas chromatographymass spectrum and high performance liquid chromatography are by trench oil decomposition, with mark
Quasi- spectrogram is contrasted, and is detected.In addition with measure electrical conductivity, viscosity, the method for dielectric constant detection gutter oil, or
The method of inspection of gutter oil particle diameter distribution in particular solution is determined, the method that gutter oil is detected using radioactivity survey, various lifes
Analyte detection method.The appearance of these methods is all because the complicated component of gutter oil, caused by the trench oil nature difference of separate sources,
Also persistently there is the detection method of various gutter oils at present.Animal oil can be typically mixed into gutter oil, contains grease in animal oil,
There can be the cholesterol more than common vegetable oil, so start with terms of cholesterol, and the effective means of detection gutter oil.Courage
The assay method of sterol has liquid chromatography, gas chromatography, thin-layered chromatography, ultraviolet-visible spectrophotometry etc., also occurs
Chemoluminescence method.Above method respectively has advantage and disadvantage, and chromatography has the shortcomings of cumbersome, the influence factor that need to be considered is more,
Although ultraviolet-visible spectrophotometry can be determined simply, qualitative analysis is difficult, influences the shape and intensity of absorption spectrum
Factor is more.
At present, it is domestic not yet to formulate the national standard method that gutter oil differentiates detection, although researcher is carried out both at home and abroad
Some explorations, differentiate that gutter oil when carrying out Physico-chemical tests, can examine such as moisture, proportion, index of refraction, saponification respectively
Value, acid number, carbonyl value, peroxide value, iodine number heavy metal, aliphatic acid are with respect to degree of unsaturation, cholesterol, residue detection, oxidation production
The indexs such as analyte detection.But it is actually rare to the report of gutter oil detection, its main cause is the trench oil component ratio of high acid value
More complicated, its detection method wants accuracy quantitatively still relatively difficult at present also in the experimental study stage.Because gutter oil has
Exogenous pollution substance characteristics, so be mixed in for dish washing detergent surfactant sodium dodecyl base benzene sulfonic acid sodium salt in gutter oil,
And edible oil is free of the phenomenon of this artificial synthesized chemical substance.Fluorescent spectrometry is mainly to detect the dodecyl in gutter oil
Benzene sulfonic acid sodium salt, in gutter oil the detection of cholesterol use high performance liquid chromatography or gas chromatography.
The content of the invention
In order to solve the above problems, an object of the present invention is the provision of one kind XRF detection gutter oil
The method of middle cholesterol.
For the above-mentioned purpose, a kind of fluorescent spectrometry of the present invention surveys the method that cholesterol level differentiates gutter oil.Including with
Lower step：
The drafting of standard curve：Take the cholesterol-CTAB aqueous solution of the prescribed concentration of gradient volume, then with isometric
The CTAB aqueous solution is diluted to the cholesterol-CTAB aqueous solution of various concentrations gradient, determines various concentrations gradient cholesterol-CTAB water
The fluorescence spectrum of solution obtains the standard curve of the cholesterol solution of cholesterol；
Sample detection：Take testing sample and qualified vegetable oil to be respectively placed in volumetric flask, in two volumetric flasks and respectively according to
The absolute ethyl alcohol of the secondary KOH solution and equivalent for adding equivalent, after shaking up, it is placed in 50 DEG C~60 DEG C thermostat water baths and carries out 4h~6h
Saponification, room temperature is cooled to afterwards, adds the n-hexane of equivalent, gently vibrate volumetric flask, rear 1~2h of stratification, by upper liquid
Pour out, repeat above-mentioned extraction process more than twice, after extract is merged, be respectively placed in glass with pipette, extract equivalent extract
In glass bottle, n-hexane in bottle is dried up with nitrogen, the CTAB solution for adding equivalent carries out fluoroscopic examination；
The fluorescent intensity that testing sample and qualified vegetable oil measure obtains testing sample and conjunction by being contrasted with standard curve
The cholesterol level of lattice vegetable oil；
The comparison of testing sample and qualified vegetable oil cholesterol level：Testing sample cholesterol level is higher than qualified vegetable oil
During cholesterol level, then contain gutter oil in testing sample.
The invention difference from existing technology is that the present invention achieves following technique effect：
The present invention is using cholesterol as the specific index for differentiating gutter oil, using XRF to predominantly detect instrument,
Complete testing conditions are constructed by repetition test, the present invention can quickly and accurately detect whether contain trench in sample
Oil, detection are limited to 0.0094g/L.
The invention will be further described below in conjunction with the accompanying drawings.
Brief description of the drawings
Fig. 1 is the fluorescence spectra of various concentrations cholesterol；
Fig. 2 is cholesterol standard working curve；
Fluorescence spectra after the processing of Fig. 3 different materials.
Embodiment
With reference to embodiments, the forgoing and additional technical features and advantages are described in more detail.
Step A, the configuration of standard liquid：
(1) due to cholesterol, solubility is small in water, thus it is by CTAB that it is solubilized, increase its solubility.Weigh
CTAB is dissolved in water, and shakes up the CTAB solution for being made into that molar concentration is 3.0~4.0mmol/L.
(2) cholesterol Standard Stock solutions：
Take cholesterol to add absolute ethyl alcohol to dissolve, shake up the cholesterol solution for being made into that mass concentration is 0.8~1.2g/L.
(3) configured good solution is pipetted into 2.5mL respectively, be respectively placed in 100mL volumetric flask, treat that ethanol is evaporated
Afterwards, scale is settled to the CTAB solution As prepared, is made into 0.025g/L cholesterol solution.Cholesterol standard serial solution：With
Pipette pipette respectively the above-mentioned cholesterol 0.2 prepared, 0.4,1.2,2.0,2.8,3.6,4.4,5.2,6.0,8.0mL it is above-mentioned
The cholesterol solution prepared is into 10mL test tube, with CTAB solution constant volumes, the concentration of cholesterol solution is respectively 0.0005,
0.001、0.003、0.005、0.007、0.009、0.011、0.013、0.015、0.02g/L。
Step B, sample treatment：
Take respectively vegetable oil, lard, gutter oil and oily edible oil and the mixed oily 2.0~4.0g of gutter oil in
In 50mL volumetric flasks, 3~5mL 0.5mol/L KOH solution and 8~12mL absolute ethyl alcohols are sequentially added.After gently shaking up, put
4h~6h saponification is carried out in 50 DEG C~60 DEG C thermostat water baths.Period shakes volumetric flask every 20~30min, makes oil sample good fortune complete
Entirely.After the completion of saponification, take out volumetric flask and be cooled to room temperature.8~10mL n-hexanes are sequentially added, gently vibrate volumetric flask, it is rear quiet
Put 1~2h of layering.Upper liquid is poured out, repeats above-mentioned extraction process twice, after extract will merge three times, use pipette, extract
5~8mL of extract is placed in vial, is dried up n-hexane in bottle with nitrogen, is added 10ml solution As and is carried out fluoroscopic examination.
Step C, the structure of XRF condition：
XRF：F2500 types, FDAC
Slit width：EX=5nm, EM=5nm, λ ex=266nm, λ em=280nm
Sweep speed：Photomultiplier tube voltage 400V
Step D, sample measure and result judge：
Under the conditions of above-mentioned fluorescence spectrum, standard curve obtained by measure cholesterol standard serial solution is calculated in solution to be measured
The content of cholesterol.
As that in testing sample at excitation wavelength is 266nm, the emission peak at 280nm can be detected, then show testing sample
In cholesterol be present, compared with qualified vegetable oil, the peak value of qualified vegetable oil if more than, then it is assumed that this oil for gutter oil or
Person is that gutter oil is mixed with vegetable oil.
Measuring principle：Commonly use qualified vegetable oil to be typically free of or containing a small amount of cholesterol, due to mixed in gutter oil
Animal oil or animal tallow are entered, wherein containing cholesterol.Although by certain processing, the content of its cholesterol can compare
It is larger, differentiate that gutter oil specificity is strong by the content of cholesterol detection.
Embodiment 1
The method that cholesterol in vegetable oil is detected with XRF, comprises the following steps：
(1) CTAB (cetyl trimethylammonium bromide) solution：CTAB0.6380g accurately is weighed, is put into 50mL beakers,
Dissolved with a small amount of distilled water, be subsequently placed in constant volume in 500mL volumetric flasks, the concentration for obtaining CTAB is 3.5mmol/L solution, i.e.,
For solution A.
(2) accurately weigh cholesterol 0.0100g, be dissolved in a certain amount of absolute ethyl alcohol, after be placed in 10mL volumetric flasks, use
Absolute ethyl alcohol is settled to graduation mark, you can it is 1.0g/L cholesterol standard liquids to obtain mass concentration.By configured good solution point
2.5mL is not pipetted, is respectively placed in 100mL volumetric flask, after ethanol is evaporated, scale is settled to the CTAB solution As prepared,
It is made into 0.025g/L cholesterol solution.
(3) cholesterol standard serial solution：Pipetted respectively with pipette the above-mentioned cholesterol 0.2 prepared, 0.4,1.2,
2.0th, 2.8,3.6,4.4,5.2,6.0, the 8.0mL above-mentioned cholesterol solution prepared is into 10mL test tube, with CTAB solution
Constant volume, the concentration of cholesterol solution is respectively 0.0005,0.001,0.003,0.005,0.007,0.009,0.011,0.013,
0.015、0.02g/L。
Step B, sample treatment
Fetch from golden dragonfish vegetable oil 4.0g in 50mL volumetric flasks, sequentially add 5mL0.5mol/lKOH solution and 12mL
Absolute ethyl alcohol.After gently shaking up, it is placed in 55 DEG C of thermostat water baths and carries out 5h saponification.Period shakes volumetric flask every 30min, makes oil
Sample good fortune is complete.After the completion of saponification, take out volumetric flask and be cooled to room temperature.8mL n-hexanes are sequentially added, gently vibrate volumetric flask,
Stratification 1h afterwards.Upper liquid is poured out, repeats above-mentioned extraction process twice, after extract will merge three times, inhaled with pipette
Take extract 5mL to be placed in vial, dried up n-hexane in bottle with nitrogen, add solution A 10ml and carry out fluoroscopic examination.
Embodiment 2
The method that cholesterol in gutter oil is detected with XRF, comprises the following steps：
(1) CTAB (cetyl trimethylammonium bromide) solution：Weigh 0.5468CTAB to be dissolved in water, shake up and be made into quality
Concentration is 3.0mmol/L CTAB solution.
(2) accurately weigh cholesterol 0.0100g, be dissolved in a certain amount of absolute ethyl alcohol, after be placed in 10mL volumetric flasks, use
Absolute ethyl alcohol is settled to graduation mark, you can it is 1.0g/L cholesterol standard liquids to obtain mass concentration.By configured good solution point
2.5mL is not pipetted, is respectively placed in 100mL volumetric flask, after ethanol is evaporated, scale is settled to the CTAB solution As prepared,
It is made into 0.025g/L cholesterol solution.
(3) cholesterol standard serial solution：Pipetted respectively with pipette the above-mentioned cholesterol 0.2 prepared, 0.4,1.2,
2.0th, 2.8,3.6,4.4,5.2,6.0, the 8.0mL above-mentioned cholesterol solution prepared is into 10mL test tube, with CTAB solution
Constant volume, the concentration of cholesterol solution is respectively 0.0005,0.001,0.003,0.005,0.007,0.009,0.011,0.013,
0.015、0.02g/L。
Step B, sample treatment
The gutter oil 2.0g from cafe is fetched in 50mL volumetric flasks, sequentially add 4mL0.5mol/lKOH solution and
10mL absolute ethyl alcohols.After gently shaking up, it is placed in 60 DEG C of thermostat water baths and carries out 4h saponification.Period shakes volumetric flask every 20min,
Make oil sample good fortune complete.After the completion of saponification, take out volumetric flask and be cooled to room temperature.10mL n-hexanes are sequentially added, gently vibration is held
Measuring bottle, rear stratification 1.5h.Upper liquid is poured out, repeats above-mentioned extraction process twice, after extract will merge three times, with shifting
Liquid pipe is drawn extract 6mL and is placed in vial, is dried up n-hexane in bottle with nitrogen, adds solution A 10ml and carries out fluorescence
Detection.
Embodiment 3
It is 1 with XRF detection gutter oil and vegetable oil mixed proportion:The method of cholesterol in when 1, including it is as follows
Step：
(1) CTAB (cetyl trimethylammonium bromide) solution：Weigh 0.7290CTAB to be dissolved in water, shake up and be made into quality
Concentration is 4.0mmol/L CTAB solution.
(2) accurately weigh cholesterol 0.0100g, be dissolved in a certain amount of absolute ethyl alcohol, after be placed in 10mL volumetric flasks, use
Absolute ethyl alcohol is settled to graduation mark, you can it is 1.0g/L cholesterol standard liquids to obtain mass concentration.By configured good solution point
2.5mL is not pipetted, is respectively placed in 100mL volumetric flask, after ethanol is evaporated, scale is settled to the CTAB solution As prepared,
It is made into 0.025g/L cholesterol solution.
(3) cholesterol standard serial solution：Pipetted respectively with pipette the above-mentioned cholesterol 0.2 prepared, 0.4,1.2,
2.0th, 2.8,3.6,4.4,5.2,6.0, the 8.0mL above-mentioned cholesterol solution prepared is into 10mL test tube, with CTAB solution
Constant volume, the concentration of cholesterol solution is respectively 0.0005,0.001,0.003,0.005,0.007,0.009,0.011,0.013,
0.015、0.02g/L。
Step B, sample treatment
It is 1 to fetch from the gutter oil of cafe and golden dragonfish vegetable oil mixed proportion:3.0g is in 50mL volumetric flasks when 1,
Sequentially add 3mL0.5mol/lKOH solution and 8mL absolute ethyl alcohols.After gently shaking up, it is placed in 50 DEG C of thermostat water baths and carries out 6h soaps
Change.Period shakes volumetric flask every 25min, makes oil sample saponification complete.After the completion of saponification, take out volumetric flask and be cooled to room temperature.According to
Secondary addition 9mL n-hexanes, gently vibrate volumetric flask, rear stratification 2h.Upper liquid is poured out, repeats above-mentioned extraction process two
It is secondary, after extract will merge three times, be placed in pipette, extract extract 8mL in vial, with nitrogen by n-hexane in bottle
Drying, add solution A 10ml and carry out fluoroscopic examination.
Embodiment 4
It is 1 with XRF detection gutter oil and vegetable oil mixed proportion:The method of cholesterol in when 9, including it is as follows
Step：
(1) CTAB (cetyl trimethylammonium bromide) solution：Weigh 0.7290CTAB to be dissolved in water, shake up and be made into quality
Concentration is 4.0mmol/L CTAB solution.
(2) accurately weigh cholesterol 0.0100g, be dissolved in a certain amount of absolute ethyl alcohol, after be placed in 10mL volumetric flasks, use
Absolute ethyl alcohol is settled to graduation mark, you can it is 1.0g/L cholesterol standard liquids to obtain mass concentration.By configured good solution point
2.5mL is not pipetted, is respectively placed in 100mL volumetric flask, after ethanol is evaporated, scale is settled to the CTAB solution As prepared,
It is made into 0.025g/L cholesterol solution.
(3) cholesterol standard serial solution：Pipetted respectively with pipette the above-mentioned cholesterol 0.2 prepared, 0.4,1.2,
2.0th, 2.8,3.6,4.4,5.2,6.0, the 8.0mL above-mentioned cholesterol solution prepared is into 10mL test tube, with CTAB solution
Constant volume, the concentration of cholesterol solution is respectively 0.0005,0.001,0.003,0.005,0.007,0.009,0.011,0.013,
0.015、0.02g/L。
Step B, sample treatment
It is 1 to fetch from the gutter oil of cafe and golden dragonfish vegetable oil mixed proportion:3.0g is in 50mL volumetric flasks when 9,
Sequentially add 3mL0.5mol/lKOH solution and 8mL absolute ethyl alcohols.After gently shaking up, it is placed in 50 DEG C of thermostat water baths and carries out 6h soaps
Change.Period shakes volumetric flask every 25min, makes oil sample saponification complete.After the completion of saponification, take out volumetric flask and be cooled to room temperature.According to
Secondary addition 9mL n-hexanes, gently vibrate volumetric flask, rear stratification 2h.Upper liquid is poured out, repeats above-mentioned extraction process two
It is secondary, after extract will merge three times, be placed in pipette, extract extract 8mL in vial, with nitrogen by n-hexane in bottle
Drying, add solution A 10ml and carry out fluoroscopic examination.
The fluorescence spectra of various concentrations cholesterol derived above is as shown in figure 1, and then obtain Fig. 2 cholesterol standard works
Make curve；Fluorescence spectra after the processing of embodiment 1-4 different materials is as shown in Figure 3.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
The various modifications and improvement that case is made, it all should fall into the protection domain of claims of the present invention determination.
Claims (1)
1. a kind of fluorescent spectrometry surveys the method that cholesterol level differentiates gutter oil, it is characterised in that comprises the following steps：
Step A, the configuration of standard liquid：
(1) weigh CTAB to be dissolved in water, shake up the CTAB solution for being made into that molar concentration is 3.0~4.0mmol/L；
(2) cholesterol Standard Stock solutions：
Take cholesterol to add absolute ethyl alcohol to dissolve, shake up the cholesterol solution for being made into that mass concentration is 0.8~1.2g/L；
(3) above-mentioned configured good cholesterol solution 2.5mL is pipetted, is placed in 100mL volumetric flask, after ethanol is evaporated, is used
The CTAB solution prepared is settled to scale, is made into 0.025g/L cholesterol solution；
Cholesterol standard serial solution：Pipetted respectively with pipette the above-mentioned 0.025g/L prepared cholesterol solution 0.2,0.4,
1.2nd, 2.0,2.8,3.6,4.4,5.2,6.0, in 8.0mL to 10mL test tube, with above-mentioned CTAB solution constant volume, cholesterol solution
Concentration be respectively 0.0005,0.001,0.003,0.005,0.007,0.009,0.011,0.013,0.015,0.02g/L；
Step B, sample treatment：
Vegetable oil, lard, gutter oil are taken respectively and are held by the mixed oily 2.0~4.0g of edible oil and gutter oil in 50mL
In measuring bottle, 3~5mL 0.5mol/L KOH solution and 8~12mL absolute ethyl alcohols are sequentially added, after gently shaking up, is placed in 50 DEG C
~60 DEG C of thermostat water baths carry out 4h~6h saponification, during which shake volumetric flask every 20~30min, make oil sample good fortune complete, soap
After the completion of change, take out volumetric flask and be cooled to room temperature, sequentially add 8~10mL n-hexanes, gently vibrate volumetric flask, rear stratification
1~2h, upper liquid is poured out, repeats above-mentioned extraction process twice, after extract will merge three times, with pipette, extract extract
5~8mL is placed in vial, is dried up n-hexane in bottle with nitrogen, is added 10ml CTAB solution and is carried out fluoroscopic examination；
Step C, the structure of XRF condition：
XRF：F2500 types, FDAC；
Slit width：EX=5nm, EM=5nm, λ ex=266nm, λ em=280nm；
Sweep speed：Photomultiplier tube voltage 400V；
Step D, sample measure and result judge：
Under the conditions of above-mentioned fluorescence spectrum, measure cholesterol standard serial solution obtains standard curve, is calculated and treated using standard curve
Survey the content of cholesterol in solution；
As testing sample excitation wavelength be 266nm at, the emission peak at 280nm can be detected, then show exist in testing sample
Cholesterol, compared with qualified vegetable oil, the peak value of qualified vegetable oil if more than, then it is assumed that this oil is either planted for gutter oil
Gutter oil is mixed with thing oil.
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| CN104949947A (en) * | 2015-06-09 | 2015-09-30 | 厦门斯坦道科学仪器股份有限公司 | Rapid edible oil quality detection method |
| CN105004804B (en) * | 2015-06-29 | 2017-06-13 | 苏州东辰林达检测技术有限公司 | Waste oil detection method |
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| CN106770123B (en) * | 2017-01-04 | 2021-06-18 | 新疆维吾尔自治区产品质量监督检验研究院 | Device and method for identifying illegal cooking oil by flow injection fluorescence method |
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| CN102645424A (en) * | 2012-03-02 | 2012-08-22 | 宁夏大学 | Method for rapidly detecting edible oil added with illegal cooking oil |
| CN102749315A (en) * | 2012-07-18 | 2012-10-24 | 滁州学院 | Method for rapidly detecting hogwash oil by synchronous fluorescence spectrum |
| CN103913435B (en) * | 2014-04-24 | 2017-02-01 | 江西农业大学 | Method and device for quickly detecting hogwash oil based on multi-source information fusion |
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